Imidazole → HCID 20286585、化合物

HRID 126879

反応式

HRID 126879 の反応式
Br[CH:2]([O:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][Cl:6].[NH:18]1[CH:22]=[CH:21][N:20]=[CH:19]1.[C:23]1([S:37]([OH:40])(=[O:39])=[O:38])[C:32]2[CH:31]=[CH:30][CH:29]=[C:28]([S:33]([OH:36])(=[O:35])=[O:34])[C:27]=2[CH:26]=[CH:25][CH:24]=1>C(#N)C.CC(C)=O>[C:23]1([S:37]([OH:40])(=[O:39])=[O:38])[C:32]2[CH:31]=[CH:30][CH:29]=[C:28]([S:33]([OH:36])(=[O:35])=[O:34])[C:27]=2[CH:26]=[CH:25][CH:24]=1.[Cl:17][C:14]1[CH:15]=[CH:16][C:11]([O:10][CH:2]([N:18]2[CH:22]=[CH:21][N:20]=[CH:19]2)[C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][Cl:6])=[CH:12][CH:13]=1

参加物

6

反応物 3

HCID 795ImidazoleHCID 66661,5-Naphthalenedisulfonic acidHCID 20286562HCID 20286562、化合物

生成物 1

HCID 20286585HCID 20286585、化合物収率 84.7%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6342Acetonitrile溶媒

実験手順

17 g (0.05 mol) of crude 1-bromo-1-(4-chlorophenoxy)-3,3-dimethyl-4-chloro-butan-2-one were dissolved in 100 ml of absolute acetonitrile. 12 g (0.175 mol) of imidazole were added to this solution and the mixture was heated under reflux for 40 hours. Thereafter, it was concentrated by distilling off the solvent in vacuo and the residue was taken up in 300 ml of methylene chloride. The methylene chloride mixture was washed three times with 100 ml of water each time, dried over sodium sulphate and concentrated again in vacuo. The residue was taken up in 100 ml of acetone, and a solution of 9 g (0.038 mol) of 1,5-naphthalenedisulphonic acid in 50 ml of acetone was added. After 2 hours, the precipitate which had formed was filtered off and dried. 19.8 g (80.7% of theory) of 1-(4-chlorophenoxy)-1-(imidazol-1-yl)-3,3-dimethyl-4-chloro-butan-2-one naphthalene-1,5-disulphonate of melting point 266°- 267° C. were obtained. ##STR14##

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 40 hours
  3. concentrationThereafter, it was concentrated
  4. distillationby distilling off the solvent in vacuo
  5. washThe methylene chloride mixture was washed three times with 100 ml of water each time
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated again in vacuo
  8. customthe precipitate which had formed
  9. filtrationwas filtered off
  10. customdried

出典と根拠

ORDレコード
ord-e16aee086878472a9e58aad7c5ba34c4
出典データセット
uspto-grants-1981_03
特許番号
US04254132

関連ノート

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